A kind of preparation method of PVDF fluorocarbon powder paints
Technical field
The present invention relates to a kind of preparation method of PVDF fluorocarbon powder paints.
Background technology
Fluorocarbon coating, as a kind of high performance coating products, is with fluorine resin as main film forming matter, and in fluororesin
On the basis of through a kind of new coating material for being modified, processing.Fluorocarbon coating is mainly characterized by resin containing a large amount of
F-C keys, bond energy is 485kJ/mol, the bond energy (413kJ/mol) far above C-H.Therefore in illumination, thermal environment or extensive chemical
Under corrosive environment, F-C keys are maintained to stable state, so as to show the weatherability of fluorocarbon coating overlength, protrusion
, used as a kind of emerging high weatherability coating, fluorocarbon coating was come out in 20th century for salt fog resistance and resistant to chemical media corrosion stability
The fifties, the anticorrosion engineering of heavy construction steel construction, the such as steel construction of stadiums, large bridge have been widely used in it
Heavy anti-corrosion paint etc..
At present, the application form of domestic fluorocarbon coating is mainly based on solvent based coating, the production of solvent-borne type fluorocarbon coating and
Construction technology is ripe, coating it is numerous it is architectural embodied very well, traction is high.With country to environmental protection increasingly
Pay attention to, using being increasingly subject to limit, coating reduces VOC emission amount as far as possible and weighs very much solvent-borne type fluorocarbon coating in first application
Will.Powdery paints VOC emission amount is very low to be more suitable for using in high-temperature baking type occasion.
Fluorocarbon powder resin kind is a lot, but it is little to apply to the kind of powdery paints.Consider from practical application angle,
Thermoplasticity and thermosetting 2 kind can be divided into by film forming matter as building material surface fluorocarbon powder resin.Thermoplastic fluoroelastomer carbon dust is applied
Material is with PVDF resins as base-material;Thermosetting fluorocarbon powder coatings are with CTFE-vinyl ethers/ester resin as base-material.
PVDF fluorocarbon powder paints occur in 20 century 70s, and FEVE fluorocarbon powder paints were opened from late 1990s
Beginning is commercially applied, and existing market occupation rate is still very low.In recent years, domestic powdery paints industry is needed to fluorocarbon powder paint
Ask more and more vigorous;External Middle East is many, and building requirement coating is without solvent and weatherability will reach AAMA2605-
2005 standards, increase to fluorocarbon powder paint demand;Asia and Oceania area have equally to fluorocarbon powder paint demand
Tendency, these market development directions are fast-developing there is provided strong impetus in building materials field to fluorocarbon powder paint.
PVDF is polyvinylidene fluoride, and PVDF fluorocarbon coatings are the top products in metal current building coats, with
Confirmed most permanent weather resistance, and with excellent resist chemical performance and excellent mechanical performance, it is nearly all
Advanced metal building all use is all fluororine-carbon coating.
But, current PVDF thermoplastic fluoroelastomers carbon coating almost all is, using solvent-borne type PVDF F-C paints, to need in solution
Middle dispensing formulations raw material.Therefore inevitably in the feed, production process and contain solvent using process.With country
Pay attention to day by day to environmental protection, due to its VOC emission problem,, using being increasingly subject to limit, coating is first for which for solvent-borne type fluorocarbon coating
Reduce VOC emission amount during secondary application as far as possible extremely important.
And some adopt aqueous PVDF thermoplastic fluoroelastomers carbon coating dispensing formulations raw material in water-based emulsion (or aqueous solution), though
So relatively above-mentioned solvent-borne type fluorocarbon coating reduces by 70% or so solvent, but still in the feed, production process and use
Process contains solvent.
Existing PVDF fluorocarbon powder paints several method shortcoming:Spray drying process, melting extrusion mixing method, and front road
Technique spray drying process postchannel process adopts melting extrusion mixing method.
1st, spray drying process:PVDF thermoplasticity F-C paints are first prepared, then PVDF fluorine carbon dusts are prepared using drying process with atomizing
Last coating.In manufacture process, in its raw material, there is solvent, production process has solvent, this technique is loaded down with trivial details, high energy consumption, also there is solvent
A series of problems, such as recycling.
2nd, melting extrusion mixing method:PVDF resins, acrylic resin, pigment, auxiliary agent, filler are adopted for raw material → high-speed stirring
Mix type mixer premixing → double screw extruder extrusion → cooling it is broken → liquid nitrogen deep is broken → classification sieves → PVDF fluorine
Fluoropolymer Powder Coatings finished product.It is poor to there is melting extrusion melting effect in this method, and extruder screw not easy cleaning, later stage also need to hold high
Expensive loaded down with trivial details liquid nitrogen frozen disintegrating process, industrial applications difficulty are larger, and domestic also no producer is produced using the method at present
PVDF fluorocarbon powder paints, no product releases market, only document introduction to this method so far.
3rd, the postchannel process of the front road technique+melting extrusion mixing method of spray drying process first prepares PVDF thermoplasticity F-C paints
→ vacuum is not exclusively drained solvent → will be pressed into sheet → just crush → drain solvent → liquid nitrogen deep into thing and crush → was classified
Sieve → PVDF fluorocarbon powder paint finished products.So far no product releases market, only document introduction to this method page.
Above-mentioned 2,3 two methods only have document introduction at present, it is impossible to volume production, trace it to its cause:Lack substantial production hand
Section, the process costs for not having perfect process facility, costliness loaded down with trivial details etc..And production process still uses solvent, inevitably
Still there is VOC emission.
The content of the invention
The present invention is solution above-mentioned technical problem, there is provided a kind of preparation method of PVDF fluorocarbon powder paints, its feature
It is to comprise the following steps:
Step 1, material is put in intelligent and high-efficiency dispersion machine, at least includes PVDF fluorocarbon resins, supporting in the material
Whether resin, inorganic pigment and auxiliary agent, the intelligent and high-efficiency dispersion machine reach pre-conditioned ginseng by the feedback parameter for detecting
Count to control scattering parameter, the scattering parameter includes main-shaft torque and material temperature, and the feedback parameter includes main-shaft torque, material temperature
Real time value and its rate of change, the pre-conditioned parameter includes the corresponding TG points of the preset value and each resin of main-shaft torque
Temperature, preset value correspondence differential responses stage of the conditional parameter at least include the first preset value, the second preset value, the 3rd pre-
If value and the 4th preset value, the control of these response parameters according to the real time value of the feedback parameter in intelligent and high-efficiency dispersion machine with
And rate of change carries out real-time adjustment;
The material release sequence and decentralised control process are as follows:PVDF fluorocarbon resins are put into first, then put into inorganic face
Material, adjusts main-shaft torque and rises high-temperature to the first preset value, keep the temperature to make inorganic pigment fully dispersed in 1~2 minute
And reunite in PVDF fluorocarbon resins, subsequent adjustment main-shaft torque to reduce temperature fully dispersed, when temperature is down to the second preset value
Auxiliary resin and auxiliary agent are put into when following, are adjusted main-shaft torque and high-temperature are risen to the 3rd preset value, keep 1~2 point of the temperature
Clock makes auxiliary resin also fully be reunited, subsequently adjustment main-shaft torque to reduce temperature fully dispersed to the 4th preset value
After discharge material;
Step 2, will be fully dispersed after material be put into banburying comminutor in continuously mediated, released, manufacture particulate matter,
Mixing temperature is controlled at 220~240 DEG C;
Particulate matter is transported to ACM grinding machines and is crushed by step 3, and in mill chamber, temperature control is at 5~17 DEG C;
Material after crushing is carried out selection by winnowing by step 4, and the particle diameter of selection by winnowing is more than 10um;
Material after selection by winnowing is carried out spheroidising by step 5, by material powders particle disposal balling-up kenel;
Step 6, the material after spheroidising is vacuum-packed, and keeps stablizing for accumulating phase quality.
Further, TG point of first preset value for PVDF fluorocarbon resins, second preset value are auxiliary resin
TG points, the 3rd preset value and the 4th preset value are 50 DEG C.
Further, also include auxiliary agent in the material, the auxiliary resin is acrylic resin or epoxy resin or poly-
Urethane resin or polyester resin.
Further, B44 acrylic resin of the acrylic resin for LG-DOW, its weight with PVDF fluorocarbon resins
Measuring proportioning is:70 parts of PVDF fluorocarbon resins, 30 parts of B44 acrylic acid tree resins.
Further, when the auxiliary resin is epoxy resin, the weight of the PVDF fluorocarbon resins and epoxy resin is matched somebody with somebody
Than for:60 parts of PVDF fluorocarbon resins, 40 parts of epoxy resin.
Further, when the auxiliary resin is polyurethane resin, the weight of the PVDF fluorocarbon resins and polyurethane resin
Measuring proportioning is:50 parts of PVDF fluorocarbon resins, 50 parts of polyurethane resin.
The manufacture process of the present invention does not contain solvent, with energy-saving and environmental protection, explosion-proof, safe, than traditional plain edition powder
The energy consumption of coating is low by 20%, low noise<85 decibels, air discharge PM2.5 pollutions are up to standard.
Specific embodiment
Most highly preferred embodiment of the invention is as follows, a kind of preparation method of PVDF fluorocarbon powder paints, comprises the following steps:
Step 1, PVDF fluorocarbon resins, acrylic resin, inorganic pigment, auxiliary agent are put in intelligent and high-efficiency dispersion machine, its
In each weight of material proportioning be:70 parts of PVDF fluorocarbon resins, 30 parts of B44 acrylic resins, inorganic pigment (1 part of cobalt blue, R706 titaniums
16 parts of white powder), auxiliary agent it is micro.
Step 1, each material is put in intelligent and high-efficiency dispersion machine, and the material release sequence and the stage of reaction are as follows:It is first
PVDF fluorocarbon resins are first put into, then puts into R706 titanium dioxides, adjust main-shaft torque and high-temperature is risen to after 85~150 DEG C, keep
The temperature makes inorganic pigment fully dispersed in 3~10 minutes and reunites in PVDF fluorocarbon resins, subsequently adjusts main-shaft torque and reduces
Temperature to less than 85~120 DEG C it is fully dispersed when, input auxiliary resin and auxiliary agent, adjustment main-shaft torque simultaneously rise high-temperature to 50
DEG C, keep the temperature to make auxiliary resin also fully be reunited in 3~10 minutes, subsequently adjust main-shaft torque and temperature is reduced to 50
Fully dispersed rear discharge material below DEG C;Wherein parameters, are controlled by the intelligent program system of connection intelligent and high-efficiency dispersion machine
Its main-shaft torque, electric current, temperature of charge etc. and the parameter such as every rate of change are made, through each sensor by the data of random acquisition
Jing engineering computer for analysis compares, then feeds back to execution system and carry out real-time adjustment.
Step 2, will be fully dispersed after material be put into banburying comminutor in continuously mediated, released, manufacture particulate matter,
Mixing temperature is controlled at 220~240 DEG C.
Particulate matter is transported to ACM grinding machines and is crushed by step 3, and in mill chamber, temperature control is at 5~17 DEG C.
Material after crushing is carried out selection by winnowing by step 4, and the particle diameter of selection by winnowing is more than 10um.
Material after selection by winnowing is carried out spheroidising by step 5, by material powders particle disposal balling-up kenel.
Material after spheroidising is carried out vacuum packaging and obtains fluorocarbon coating finished product, keeps accumulating phase quality by step 6
It is stable.
The control process of wherein intelligent and high-efficiency dispersion machine is summarized as:Cold dispersion (PVDF fluorocarbon resins) → heat bonding (PVDF
Fluorocarbon resin and inorganic pigment are reunited) → cold dispersion (auxiliary resin and PVDF fluorocarbon resins) → heat bonding (auxiliary resin with
PVDF fluorocarbon resins are reunited) → cold discharge.And PVDF fluorocarbon resins are evenly distributed on containing pigment, auxiliary agent propylene in the process
In the copolymerization suspension system of acid resin nanoscale or Subnano-class, and make them in each resin TG points (vitrification point) with
Formation reunion compound of the PVDF fluorocarbon resins particle for core, redisperse is particle, forms (the dispersion of PVDF fluorocarbon powder paints
Agent is air).
Above-described embodiment provide fluorocarbon coating after testing, with good dry type adhesive force, wet type adhesive force, boiling water formula
Adhesive force, pressure boiling water formula adhesive force, anti-impact force, resistance to nitric acid, resistance to hydrochloric acid, resistance to mortar, croop property are good, and glossiness is
25-40, pencil hardness are 2h, butanone is wiped and reached 160 times, meet the quality mark of GB GB5237.5 and U.S. AAMA2605
It is accurate.
Fluorocarbon coating provided by the present invention is heat-insulation energy-saving fluorocarbon coating, based on specific PVDF,
Color stuffing is compounded according to a certain ratio and is formed using isolation-type, reflection-type and radiation type heat-insulation functional stuffing, makes obstruct, radiation, anti-
The heat-insulated effect of collaboration of emitting thermal insulating filling is more preferably played.Not only effect of heat insulation is excellent for the fluorocarbon coating of preparation, and comprehensive
Excellent performance, can be effectively improved work living environment, energy saving and improve residential security, comfortableness.
In other embodiments, filled a prescription based on PVDF fluorocarbon resins, auxiliary resin can also be epoxy resin, poly- ammonia
Ester resin, polyester resin, inorganic pigment are also corresponded to and can be selected as needed, according to different auxiliary resins and inorganic pigment pair
Each weight of material proportioning is adjusted accordingly, and these simply change also in present inventive concept scope.
During using fluorocarbon coating provided by the present invention, need to be through spraying, roasting procedure, i.e. fusing, family status, film forming.Most
Coating structure after whole PVDF fluorocarbon powder paints solidification and the coating structure after the solidification of solvent type PVDF F-C paints are very
Approximate, and without the minimal residue thing stayed after solvent or water volatilization.The present invention raw material, manufacture and using process not
Containing solvent, with energy-saving and environmental protection, explosion-proof, safe, low noise lower by 20% than the energy consumption of traditional plain edition powdery paints<85 points
Shellfish, air discharge PM2.5 pollutions are up to standard.
Above in conjunction with being exemplarily described to the present invention, it is clear that the present invention is implemented and do not limited by aforesaid way
System, if the improvement of the various unsubstantialities that method of the present invention design and technical scheme are carried out is employed, or not improved general
The design and technical scheme of the present invention directly applies to other occasions, within protection scope of the present invention.